CN114974919A - Plasma nitrogen injection TiO 2 TiN electrode and preparation method and application thereof - Google Patents
Plasma nitrogen injection TiO 2 TiN electrode and preparation method and application thereof Download PDFInfo
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- CN114974919A CN114974919A CN202210606014.2A CN202210606014A CN114974919A CN 114974919 A CN114974919 A CN 114974919A CN 202210606014 A CN202210606014 A CN 202210606014A CN 114974919 A CN114974919 A CN 114974919A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000002347 injection Methods 0.000 title claims abstract description 11
- 239000007924 injection Substances 0.000 title claims abstract description 11
- 238000005468 ion implantation Methods 0.000 claims abstract description 29
- 239000002071 nanotube Substances 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 150000002500 ions Chemical class 0.000 claims description 20
- 230000001133 acceleration Effects 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
- 230000001629 suppression Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000012010 growth Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000007709 nanocrystallization Methods 0.000 abstract description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000002513 implantation Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000010849 ion bombardment Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002482 conductive additive Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000034655 secondary growth Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of electrochemistry, and discloses plasma nitrogen injection TiO 2 A TiN electrode and a preparation method and application thereof. The plasma nitrogen-injected TiO 2 The preparation method of the TiN electrode comprises the following steps: (1) taking a Ti sheet as an anode and a stainless steel sheet as a cathode, and carrying out electrochemical anodic oxidation to obtain TiO 2 A nanotube array; (2) vacuumizing an ion implanter, taking nitrogen as working gas, and carrying out TiO treatment obtained in the step (1) 2 The nanotube array is N-doped by ion implantation to obtain TiO 2 a/TiN nanotube array. The invention adopts the ion implantation mode to introduce the conductive phase TiN into the TiO 2 In the nanotube structure, material nanocrystallization and a surface activation technology are combined. Growth of surface film layer by thermal effect in N ion implantation process and high-energy ionsBombardment damage to surface film layer 2 The surface appearance of the/TiN electrode.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to plasma nitrogen injection TiO 2 TiN electrode and preparation method and application thereof
Background
Electrochemical capacitors (also known as supercapacitors) represent an emerging energy storage technology that can provide high power density, cycle life, charge rate, and good safety, among other things. The electrodes constructed by the oriented nanotube arrays are arranged perpendicular to the collector, and can easily prepare a network structure with large surface area, high stacking density and order, and the morphological characteristic of high specific surface area can promote the rapid charge/discharge performance, so that the power density is improved. Because the nanotube array is in direct contact with the current collector, the use of conductive additives and binders can be reduced, the quality of the electrode can be reduced, and the mass specific capacitance can be improved. TiO 2 2 The nano tube has higher chemical stability, strong catalytic activity and large comparative area, and can provide an excellent path for electron transmission. But TiO 2 2 As a wide bandgap semiconductor, the conductivity is relatively poor, limiting its application in supercapacitors.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a plasma nitrogen injection TiO 2 A preparation method of a TiN electrode.
The invention also aims to provide the plasma nitrogen-injected TiO prepared by the method 2 TiN electrode
It is still another object of the present invention to provide the plasma-implanted nitrogen-containing TiO 2 Application of a/TiN electrode in preparation of a super capacitor.
The purpose of the invention is realized by the following scheme:
plasma nitrogen injection TiO 2 The preparation method of the TiN electrode comprises the following steps:
(1) taking a Ti sheet as an anode and a stainless steel sheet as a cathode, and carrying out electrochemical anodic oxidation to obtain TiO 2 A nanotube array;
(2) vacuumizing an ion implanter, taking nitrogen as working gas, and carrying out TiO treatment obtained in the step (1) 2 The nanotube array is N-doped by ion implantation to obtain TiO 2 a/TiN nanotube array.
Before electrochemical anodic oxidation is carried out, firstly, ultrasonically cleaning pure titanium foil in acetone, absolute ethyl alcohol and water in sequence to remove oil stains on the surface of the titanium foil, then, placing the titanium foil in the absolute ethyl alcohol for sealing and storing, and taking out and drying before use.
The voltage of the anodic oxidation in the step (1) is 30V-50V, and the anodic oxidation time is 0.5-1 h. The electrolyte is ethylene glycol and H 2 O and NH 4 And F, mixed solution.
N ion implantation dosage is 0.1 × 10 in the step (2) of ion implantation 17 ～×20 17 ions·cm -2 Preferably 5X 10 17 ～15.0×10 17 ions·c - m 2 More preferably 10.0X 10 17 ions·cm -2 。
The ion implantation in the step (2) is specifically set as follows: the filament current of the gas source is 8-12A, the gas supply flow is 2.0-7.0 SCCM, the arc voltage is 60-80V, the arc current is 0.05-0.2A, the extraction voltage is 0.5-2 kV, the extraction current is 2-8 mA, the suppression voltage is 0.5-2 kV, the suppression current is 0.1-1 mA, the acceleration voltage is 50-70 kV, and the acceleration current is 2-8 mA.
The ion implantation in the step (2) is specifically set as follows: the filament current of the gas source is 10A, the gas supply flow is 5.0SCCM, the arc voltage is 70V, the arc current is 0.1A, the extraction voltage is 1.5kV, the extraction current is 5mA, the suppression voltage is 1kV, the suppression current is 0.5mA, the acceleration voltage is 60kV, and the acceleration current is 5 mA.
Plasma nitrogen injection TiO 2 the/TiN electrode is prepared by the method.
The above-mentioned plasma nitrogen-injected TiO 2 The application of the/TiN electrode in the preparation of the super capacitor.
Compared with the prior art, the invention has the following advantages and beneficial effects:
introducing conductive phase TiN into TiO by adopting ion implantation mode 2 In the nanotube structure, the material nanocrystallization and surface activation technology are combined to prepare TiO 2 A TiN electrode. The heat effect in the N ion implantation process affects the growth of the surface film layer and the bombardment damage of high-energy ions to the surface film layer 2 The surface appearance of the/TiN electrode. The formation of TiN phase is beneficial to reducing the resistivity, and the acicular structure appearing at the top end of the nanotube is beneficial to improving the electrochemical performance.
Drawings
FIG. 1 is an anodized TiO 2 SEM image of nanotube array, wherein (a) is TiO 2 Front view of nanotube (b) is TiO 2 Nanotube cross-sectional view
FIG. 2 shows that the N ion implantation dose is 10.0 × 10 17 ions·cm -2 Of TiO 2 2 SEM image of/TiN electrode; wherein (a) is TiO 2 The positive view (b) of the/TiN electrode is TiO 2 Sectional view of/TiN electrode.
FIG. 3 shows different doses of TiO implanted with N ions 2 CV curve of/TiN electrode (100mV/s)
FIG. 4 shows different doses of TiO implanted with N ions 2 GCD curve of TiN electrode.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Example 1
Plasma nitrogen-injected TiO 2 The preparation method of the TiN electrode comprises the following steps:
(1) preparation of TiO by two-electrode electrochemical anodic oxidation 2 And (3) a nanotube array, wherein before anodic oxidation, TA1 pure titanium foil is sequentially subjected to ultrasonic cleaning in acetone, absolute ethyl alcohol and deionized water for 10min to remove oil stains on the surface of the titanium foil, and then the titanium foil is placed in the absolute ethyl alcohol for sealing and storage, and is taken out and dried before use. The pretreated Ti sheet is used as an anode, the stainless steel sheet is used as a cathode, and the electrolyte is ethylene glycol (97.7 wt%) + H 2 O(2.0wt％)+NH 4 F (0.3 wt%). The numerical control power supply provides working voltage and controls the TiO by adjusting the voltage and time 2 Structure of nanotube arrays. And (4) taking out the Ti sheet after the anode oxidation is finished, and washing the Ti sheet with ethanol. The anodic oxidation voltage was 40V and the anodic oxidation time was 1 h.
(2) Before N ion implantation, the method comprisesThe sample was dried. The ion implanter is vacuumized to 2.5X 10 -3 And after Pa, N ion implantation is carried out. The working gas is nitrogen, and the specific setting is as follows: the filament current of the gas source is 10A, the gas supply flow is 5.0SCCM, the arc voltage is 70V, the arc current is 0.1A, the extraction voltage is 1.5kV, the extraction current is 5mA, the suppression voltage is 1kV, the suppression current is 0.5mA, the acceleration voltage is 60kV, and the acceleration current is 5 mA. Oxidizing the anodized TiO 2 The nanotube array is N-doped by ion implantation with an accelerating voltage of 60kV and N ion implantation doses of 0.5 × 10 17 、1.0×10 17 、5.0×10 17 、10.0×10 17 、20.0×10 17 ions·cm -2 To obtain TiO 2 a/TiN nanotube array.
As can be seen from FIG. 2, the dose for N implantation reaches 10.0 × 10 17 ions·cm -2 When the nano-tube is used, the top end of the nano-tube presents a typical nano-needle array structure. The method is likely to cause that the tube end receives a larger amount of ion bombardment action in unit time along with the increase of the implantation dosage and the extension of the implantation time, and secondary growth occurs under the dual action of the ion bombardment damage action and the film layer growth; from the sectional view, the structure of the top end of the nanotube becomes rough, the needle tip is long and thin, the tube wall near the proximal port is obviously damaged, and the diameter of the nanoneedle is about 50 nm.
Compared with the unmodified sample, the resistivity of the sample modified by N ion implantation is reduced in general, and is reduced to 2.46 multiplied by 10 from 523.7 omega cm of the sample which is not modified by the ion implantation -3 Ω · cm, the resistivity drops by 5 orders of magnitude. The modification by N ion implantation has a certain destructive effect, and although the relative ratio surface area is increased to a certain extent by the ion implantation, more N ions enter a material subsurface layer to form a new phase, so that the overall conductivity is increased. The introduction of the conductive substance on the surface of the material plays a positive role in the conductivity of the surface of the electrode material.
As can be seen from FIG. 3, TiO 2 The CV curve of the/TiN electrode is in a rectangular shape, which is a good embodiment of the capacitance performance. The implantation dose of N ions is 10.0 × 10 17 ions·cm -2 Is most suitably determined by a CV curveThe specific capacitance is calculated to be 19272.4mF cm -3 The specific capacitance is improved by 379.5% compared with that without injection.
The specific capacitance of the electrode without N ion injection modification is 65.7m F cm -3 . The specific capacitance corresponding to different N implantation doses is 5377.1, 7625.8, 7500.1, 24822.7 and 12261.9m F cm -3 。10.0×10 17 ions·cm -2 The specific capacitance of the sample increased by about 380.3% over that before the injection.
Modified TiO pair by N ion implantation 2 The conductivity of the/TiN electrode is obviously improved, the improvement of the conductivity is beneficial to the rapid transmission and transfer of charges in the electrochemical reaction process, the CV curve area is obviously increased, the electrochemical activity of the electrode is obviously enhanced, and the capacitance performance is effectively improved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (10)
1. Plasma nitrogen injection TiO 2 The preparation method of the TiN electrode is characterized by comprising the following steps:
(1) taking a Ti sheet as an anode and a stainless steel sheet as a cathode, and carrying out electrochemical anodic oxidation to obtain TiO 2 A nanotube array;
(2) vacuumizing an ion implanter, taking nitrogen as working gas, and carrying out TiO treatment obtained in the step (1) 2 The nanotube array is N-doped by ion implantation to obtain TiO 2 a/TiN nanotube array.
2. The production method according to claim 1, characterized in that:
n ion implantation dosage is 0.1 × 10 in the step (2) of ion implantation 17 ～×20 17 ions·cm -2 。
3. The method of claim 1, wherein:
n ion implantation dosage is 5 × 10 during ion implantation in step (2) 17 ～15.0×10 17 ions·c - m 2 。
4. The method of claim 1, wherein:
n ion implantation dosage is 10.0 × 10 in the step (2) of ion implantation 17 ions·cm -2 。
5. The method of claim 1, wherein: the voltage of the anodic oxidation in the step (1) is 30V-50V, and the anodic oxidation time is 0.5-1 h.
6. The method of claim 1, wherein: the ion implantation in the step (2) is specifically set as follows: the filament current of the gas source is 8-12A, the gas supply flow is 2.0-7.0 SCCM, the arc voltage is 60-80V, the arc current is 0.05-0.2A, the extraction voltage is 0.5-2 kV, the extraction current is 2-8 mA, the suppression voltage is 0.5-2 kV, the suppression current is 0.1-1 mA, the acceleration voltage is 50-70 kV, and the acceleration current is 2-8 mA.
7. The method of claim 1, wherein: the ion implantation in the step (2) is specifically set as follows: the filament current of the gas source is 10A, the gas supply flow is 5.0SCCM, the arc voltage is 70V, the arc current is 0.1A, the extraction voltage is 1.5kV, the extraction current is 5mA, the suppression voltage is 1kV, the suppression current is 0.5mA, the acceleration voltage is 60kV, and the acceleration current is 5 mA.
8. The method of claim 1, wherein: before electrochemical anodic oxidation is carried out, firstly, ultrasonically cleaning pure titanium foil in acetone, absolute ethyl alcohol and water in sequence to remove oil stains on the surface of the titanium foil, then, placing the titanium foil in the absolute ethyl alcohol for sealing and storing, and taking out and drying before use.
9. One kindIonic nitrogen-injected TiO 2 A/TiN electrode, prepared by the method of any one of claims 1 to 8.
10. The TiO of claim 9 plasma-implanted with nitrogen 2 The application of the/TiN electrode in the preparation of the super capacitor.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422725A (en) * | 2007-11-02 | 2009-05-06 | 中国科学院过程工程研究所 | Preparation method and use of visible light responsive nitrogen-doped titanium dioxide nano-tube |
| CN102544375A (en) * | 2011-12-30 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Wide-spectral-response flexible photo-anode of solar cell and manufacturing method of wide-spectral-response flexible photo-anode |
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- 2022-05-31 CN CN202210606014.2A patent/CN114974919A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422725A (en) * | 2007-11-02 | 2009-05-06 | 中国科学院过程工程研究所 | Preparation method and use of visible light responsive nitrogen-doped titanium dioxide nano-tube |
| CN102544375A (en) * | 2011-12-30 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Wide-spectral-response flexible photo-anode of solar cell and manufacturing method of wide-spectral-response flexible photo-anode |
Non-Patent Citations (1)
| Title |
|---|
| XUEMEI ZHOU ET AL: "TiO2 Nanotubes: Nitrogen-Ion Implantation at Low Dose Provides Noble-Metal-Free Photocatalytic H2-Evolution Activity", 《ANGEWANDTE CHEMIE-INTERNATIONAL EDITION》, vol. 55, no. 11 * |
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